CN110643362B - Tungstate up-conversion luminescent material and preparation method and application thereof - Google Patents
Tungstate up-conversion luminescent material and preparation method and application thereof Download PDFInfo
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Abstract
The application discloses a tungstate up-conversion luminescent material, a preparation method and an application thereof, and relates to the technical field of luminescent materials2‑2x‑ 2yEr2xYb2yW3O12Wherein A is one or more of elements Al, Bi, Y, Lu, La, Gd and Dy, 0<x+y<1. The application solves the problem that the existing up-conversion luminescent material can not realize the regulation and control of the luminescent performance in real time and in situ, and realizes the random regulation and control of the luminescent intensity of the up-conversion luminescent material through temperature.
Description
Technical Field
The application relates to the technical field of luminescent materials, in particular to a tungstate up-conversion luminescent material and a preparation method and application thereof.
Background
A rare earth doped up-conversion luminescent material is a photoluminescent material that is capable of converting multiple longer wavelength photons (low energy) into shorter wavelength photons (high energy). The nonlinear optical characteristic has unique advantages in many fields and high value, and the application mainly comprises a high-performance blue-green laser, biological cell optical imaging, a high-efficiency solar cell, a temperature sensor, 3D imaging and the like.
In general, rare earth doped up-conversion luminescent materials generally consist of three parts: a host material providing a suitable crystal field for the luminescent centers; activators, which absorb energy and produce luminescence by transition; dopant ions capable of absorbing and efficiently transferring energy to an activator and ultimately improving overall luminous efficiency are referred to as sensitizers. Generally, the upconversion luminescence intensity is determined by luminescence absorption and conversion efficiency. The up-conversion light absorption efficiency is mainly determined by the light scattering cross section of the dopant ions, the transparency of the matrix, and the like. The up-conversion efficiency depends on the rare-earth ion excited state dynamics and the interaction between the rare-earth ion excited state dynamics and the matrix.
At present, the regulation and control of luminescence are mainly realized by regulating the types of doped ions, regulating the concentration of the doped ions, and regulating the crystalline phase, the crystal size, the core-shell structure and the like of a matrix. However, the conventional luminescence regulation and control method cannot realize real-time and in-situ luminescence performance regulation and control.
Disclosure of Invention
The embodiment of the application provides the tungstate upconversion luminescent material and the preparation method and application thereof, solves the problem that the existing upconversion luminescent material cannot realize real-time and in-situ luminescent performance regulation and control, and realizes that the luminescent intensity of the upconversion luminescent material is regulated and controlled at will through temperature.
In order to achieve the above purpose, the present application mainly provides the following technical solutions:
in one aspect, the present application provides a tungstate upconversion luminescent material with a chemical formula of a2-2x- 2yEr2xYb2yW3O12Wherein A is one or more of elements Al, Bi, Y, Lu, La, Gd and Dy, 0<x+y<1。
Preferably, 0< x.ltoreq.0.1 and 0< y.ltoreq.0.4.
Preferably, x is 0.02 and y is 0.18.
Preferably, the particle size of the tungstate upconversion luminescent material is 0.2-100 μm.
On the other hand, the embodiment of the application provides a preparation method of a tungstate up-conversion luminescent material, which comprises the following steps:
a-containing compound, Er-containing compound, Yb-containing compound and W-containing compound were mixed according to A: er: yb: w ═ 2-2x-2 y: 2 x: 2 y: 3, pre-burning and grinding the mixture after the mixture is uniformly mixed, calcining the ground powder, cooling and grinding the powder to obtain the tungstate up-conversion luminescent material; wherein A is one or more of elements Al, Bi, Y, Lu, La, Gd and Dy, and 0< x + Y < 1.
Preferably, the chemical formula of the tungstate upconversion luminescent material is A2-2x-2yEr2xYb2yW3O12。
Preferably, 0< x.ltoreq.0.1 and 0< y.ltoreq.0.4.
Preferably, x is 0.02 and y is 0.18.
Preferably, the a-containing compound, Er-containing compound, Yb-containing compound and W-containing compound are each selected from the corresponding oxides, carbonates, oxalates, acetates or compounds present in the form of hydroxides.
Preferably, the a-containing compound, Er-containing compound and Yb-containing compound are each selected from the corresponding oxides; the W-containing compound is WO3。
Preferably, the A-containing compound, the Er-containing compound, the Yb-containing compound and the W-containing compound each have a purity of 99.99%.
Preferably, the particle size of the tungstate upconversion luminescent material is 0.2-100 μm.
Preferably, the a-containing compound, the Er-containing compound, the Yb-containing compound, and the W-containing compound are uniformly mixed by mechanical ball milling or a sol-gel method.
Preferably, the pre-sintering temperature is 400-700 ℃, and the pre-sintering time is 2-30 hours.
Preferably, the pre-sintering temperature is 600 ℃, and the pre-sintering time is 10 hours.
Preferably, the containers used for the pre-firing and the calcining are ceramic or corundum boats.
Preferably, the calcining atmosphere is air or pure oxygen, the calcining temperature is 1000-1250 ℃, and the calcining time is 2-10 hours.
Preferably, the temperature of the calcination is 1100 ℃, and the time of the calcination is 6 hours.
The embodiment of the application also provides application of the tungstate upconversion luminescent material in the fields of high-temperature upconversion imaging, temperature sensors and laser anti-counterfeiting.
One or more technical solutions provided in the embodiments of the present application have at least the following technical effects or advantages:
the tungstate upconversion luminescent material provided by the application adopts A2W3O12The type tungstate material is used as a substrate of the luminescent material, and breaks through the performance of light weakening caused by the temperature rise of the conventional up-conversion luminescent material by utilizing the negative thermal expansion performance and erbium-ytterbium co-doping, so that the performance of light enhancement caused by the temperature rise of the material is realized, the position of the luminescent peak of the material is not changed along with the change of the luminescent intensity, but the luminescent intensity is rapidly enhanced along with the temperature rise. In addition, the tungstate upconversion luminescent material has good chemical stability and high quenching concentration during rare earth doping. The luminescent material creates good conditions for regulating and controlling the luminescent performance by regulating the temperature, and has the potential of being applied to high-temperature up-conversion imaging, high-temperature and high-sensitivity temperature sensors, laser anti-counterfeiting and other aspects.
Drawings
FIG. 1 shows a luminescent material Y obtained in example 1 of the present application2-0.4Er0.04Yb0.36W3O12XRD pattern of (a);
FIG. 2 shows a luminescent material Y obtained in example 1 of the present application2-0.4Er0.04Yb0.36W3O12The normal temperature luminescence spectrogram;
FIG. 3 shows a luminescent material Y obtained in example 1 of the present application2-0.4Er0.04Yb0.36W3O12Luminescence spectra at different temperatures;
FIG. 4 shows a luminescent material Lu obtained in example 1 of the present application2-0.4Er0.04Yb0.36W3O12Graph of luminescence intensity at specific luminescence peaks (524 and 560nm) as a function of temperature;
FIG. 5 shows a luminescent material Lu obtained in example 2 of the present application2-0.4Er0.04Yb0.36W3O12The normal temperature luminescence spectrogram;
FIG. 6 shows a luminescent material Lu obtained in example 2 of the present application2-0.4Er0.04Yb0.36W3O12Up-converting luminescence spectra at different temperatures;
FIG. 7 shows a luminescent material Lu obtained in example 2 of the present application2-0.4Er0.04Yb0.36W3O12Spectra of intensity at different luminescence peak positions as a function of temperature.
Detailed Description
The present invention will be described in further detail with reference to the following examples, which are not intended to limit the invention thereto.
The tungstate luminescent material refers to WO containing anionic groups6-Or WO4-The inorganic compound of (1). Compared with other inorganic compounds, tungstate has excellent high-temperature property and good chemical and electrochemical stability, and tungstate has stronger light absorption peaks in an ultraviolet region and a near-ultraviolet region, so that tungstate is widely applied to the field of solid luminescence. At present, the field of luminescent materials mainly focuses on scheelite (CaWO)4) Type A2BWO6(A, B ═ Ca, Sr, Ba, etc.) and A2WO6(a ═ Y, Gd, Bi) type of these three structures. The three structures have excellent luminous thermal stability and very high quenching concentration, and are very excellent down-conversion luminescent materials. In addition to the tungstate materials mentioned above, there is also A2W3O12The material of tungstate, because of its larger phonon energy and lower corresponding luminous intensity, A2W3O12Type tungstate materials are rarely used as a host for luminescent materials. And the study shows that A2W3O12The tungstate material has obvious negative thermal expansion performance, and can realize zero expansion performance of the material after being compounded with some positive expansion performance materials.
This application adopts A2W3O12The type tungstate material is used as a substrate of the luminescent material, and breaks through the performance of the conventional up-conversion luminescent material that the luminescence is weakened when the temperature is increased by utilizing the negative thermal expansion performance of the type tungstate material and by erbium-ytterbium co-doping, so that the performance of the luminescent enhancement when the temperature is increased is realized, the position of the luminescent peak of the material is not changed along with the change of the luminescent intensity, but the luminescent intensity is rapidly enhanced along with the temperature increase. The luminescent material creates good conditions for regulating and controlling the luminescent performance by regulating the temperature, and has the potential of being applied to high-temperature up-conversion imaging, high-temperature and high-sensitivity temperature sensors, laser anti-counterfeiting and other aspects.
The chemical general formula of the tungstate upconversion luminescent material provided by the embodiment of the application is A2-2x-2yEr2xYb2yW3O12Wherein A is one or more of Al, Bi, Y, Lu, La, Gd and Dy, 0<x+y<1. Preferably, 0<x≤0.1，0<y is less than or equal to 0.4. More preferably, x is 0.02 and y is 0.18.
The particle size of the tungstate upconversion luminescent material is 0.2-100 mu m.
The embodiment of the application also provides a preparation method of the tungstate upconversion luminescent material, which comprises the following steps:
a compound, Er compound, Yb compound and W compound are mixed according to the proportion of A: er: yb: w ═ 2-2x-2 y: 2 x: 2 y: 3, pre-burning and grinding the mixture after the mixture is uniformly mixed, calcining the ground powder, cooling and grinding the powder to obtain the tungstate up-conversion luminescent material; wherein A is one or more of elements Al, Bi, Y, Lu, La, Gd and Dy, and 0< x + Y < 1.
Preferably, 0< x.ltoreq.0.1, 0< y.ltoreq.0.4. More preferably, x is 0.02 and y is 0.18.
The chemical general formula of the tungstate up-conversion luminescent material is A2-2x-2yEr2xYb2yW3O12。
Wherein the A-containing compound, the Er-containing compound, the Yb-containing compound and the W-containing compoundThe compounds are selected from the corresponding oxides, carbonates, oxalates, acetates or compounds in the form of hydroxides. Preferably, the a-containing compound, the Er-containing compound and the Yb-containing compound are each selected from the corresponding oxides; the W-containing compound is WO3(ii) a And the purities of the raw materials are all 99.99%.
In the preparation method, the compound containing A, the compound containing Er, the compound containing Yb and the compound containing W are uniformly mixed by a mechanical ball milling method or a sol-gel method.
In the preparation method, the presintering temperature is 400-700 ℃, and the presintering time is 2-30 hours. Preferably, the temperature of the pre-firing is 600 ℃ and the time of the pre-firing is 10 hours.
In the preparation method, the containers used for pre-burning and calcining are ceramic boats or corundum boats.
In the preparation method, the calcining atmosphere is air or pure oxygen, the calcining temperature is 1000-1250 ℃, and the calcining time is 2-10 hours. Preferably, the temperature of calcination is 1100 ℃ and the time of calcination is 6 hours.
The tungstate upconversion luminescent material can be applied to high-temperature upconversion imaging, temperature sensors and the laser anti-counterfeiting field.
The preparation method of the tungstate upconversion luminescent material is illustrated by the following specific examples.
Example 1
(1) According to the formula Y2-0.4Er0.04Yb0.36W3O12In the stoichiometric ratio of Y, Er, Yb and W, weighing Y2O3，Yb2O3，WO3And Er2O3The purity of the raw materials is 99.99 percent according to the corresponding mass, and the raw materials are ground for 2 to 3 times by absolute ethyl alcohol to be uniformly mixed;
(2) placing the ground sample in an oven at 80 ℃ for two hours for drying, then placing the sample in a corundum boat, placing the corundum boat with the sample in a high-temperature furnace for presintering, preserving heat for 6 hours at 500 ℃ in air atmosphere, and then naturally cooling to normal temperature;
(3) taking out the sample from the high-temperature furnace, grinding the sample for 2 to 3 times by using alcohol, and drying the sample;
(4) and putting the dried sample into a corundum boat, putting the corundum boat into a high-temperature furnace for calcining, slowly heating to 1100 ℃ in the air atmosphere, preserving the temperature for 6 hours, naturally cooling, and finally grinding to obtain the tungstate up-conversion luminescent material.
The particle size of the tungstate upconversion luminescent material is 0.2-100 mu m through detection.
Carrying out XRD detection on the tungstate up-conversion luminescent material prepared in the example 1 to obtain an XRD spectrogram shown in figure 1; wherein the upper part of FIG. 1 is Y2-0.4Er0.04Yb0.36W3O12X-ray diffraction spectrum of luminescent material sample with Y below2W3O12Standard cards of material. As can be seen from FIG. 1, Y prepared in example 12-0.4Er0.04Yb0.36W3O12The luminescent material being phase-pure Y2W3O12The structure, Er and Yb doping, did not significantly change the material structure.
The tungstate up-conversion luminescent material prepared in example 1 was subjected to a luminescence property test to obtain luminescence spectra shown in fig. 2, 3 and 4.
FIG. 2 shows a luminescent material Y2-0.4Er0.04Yb0.36W3O12The normal temperature luminescence spectrogram under 980nm laser excitation can be seen from FIG. 2, and the luminescent material Y is obtained under normal temperature2-0.4Er0.04Yb0.36W3O12Emitting green light under the irradiation of near infrared laser;
FIG. 3 shows a luminescent material Y under different temperature conditions2-0.4Er0.04Yb0.36W3O12A luminescence spectrum under 980nm laser excitation; as can be seen from FIG. 3, the luminescent material Y2-0.4Er0.04Yb0.36W3O12Does not change with the increase of temperature, but the luminous intensity increases with the increase of temperature.
FIG. 4 shows a luminescent material Y2-0.4Er0.04Yb0.36W3O12Graph of luminescence intensity at specific luminescence peaks (524 and 560nm) as a function of temperature; as can be seen from FIG. 4, the luminescent material Y2-0.4Er0.04Yb0.36W3O12The luminous enhancement quantity at different luminous peak positions has larger difference, and the luminous intensity with the peak position of 524nm changes most obviously along with the temperature.
As can be seen from the above, the luminescent material Y2-0.4Er0.04Yb0.36W3O12Has the property of light enhancement at the temperature rise which is different from that of the conventional material, the position of the luminescence peak of the material does not change with the change of the luminescence intensity, but the luminescence intensity rapidly increases with the temperature rise. Therefore, the tungstate upconversion luminescent material prepared by the embodiment can realize real-time and in-situ luminescent property regulation and control by randomly regulating and controlling the luminescent intensity of the upconversion luminescent material through temperature.
Example 2
(1) According to the chemical formula Lu2-0.4Er0.04Yb0.36W3O12Weighing Lu according to the stoichiometric ratio of Lu, Er, Yb and W2O3，Yb2O3，WO3And Er2O3The purity of the raw materials is 99.99 percent according to the corresponding mass, and the raw materials are ground for 2 to 3 times by absolute ethyl alcohol to be uniformly mixed.
(2) And placing the ground sample in an oven at 80 ℃ for two hours for drying, then placing the sample in a corundum boat, placing the corundum boat with the sample in a high-temperature furnace for presintering, preserving the heat for 6 hours at 500 ℃ in the air atmosphere, and then naturally cooling to the normal temperature.
(3) Taking out the sample from the high-temperature furnace, grinding the sample for 2 to 3 times by using alcohol, and drying the ground sample.
(4) And putting the dried sample into a corundum boat, putting the corundum boat into a high-temperature furnace for calcining, slowly heating to 1150 ℃ in the air atmosphere, preserving the temperature for 6 hours, naturally cooling, and finally grinding to obtain the tungstate up-conversion luminescent material.
The particle size of the tungstate upconversion luminescent material prepared by the method is 0.2-100 mu m through detection.
The tungstate up-conversion luminescent material prepared in example 2 was subjected to a luminescent property test to obtain luminescent spectra shown in fig. 5, 6 and 7.
FIG. 5 shows a luminescent material Lu2-0.4Er0.04Yb0.36W3O12The normal temperature luminescence spectrogram under the excitation of 980nm laser can be seen from FIG. 5, and the luminescent material Lu is obtained under the normal temperature condition2-0.4Er0.04Yb0.36W3O12Emitting green light under the irradiation of near infrared laser;
FIG. 6 shows the luminescent material Lu under different temperature conditions2-0.4Er0.04Yb0.36W3O12A luminescence spectrum under 980nm laser excitation; as can be seen from FIG. 6, the luminescent material Lu2-0.4Er0.04Yb0.36W3O12Does not change with the increase of temperature, but the luminous intensity increases with the increase of temperature.
FIG. 7 shows a luminescent material Lu2-0.4Er0.04Yb0.36W3O12Graph of luminescence intensity at specific luminescence peaks (524 and 560nm) as a function of temperature; as can be seen from FIG. 6, the luminescent material Lu2-0.4Er0.04Yb0.36W3O12The luminous enhancement quantity at different luminous peak positions has larger difference, and the luminous intensity with the peak position of 524nm changes most obviously along with the temperature.
As can be seen from the above, the luminescent material Lu2-0.4Er0.04Yb0.36W3O12Has the property of light enhancement at the temperature rise which is different from that of the conventional material, the position of the luminescence peak of the material does not change with the change of the luminescence intensity, but the luminescence intensity rapidly increases with the temperature rise. Therefore, the tungstate upconversion luminescent material prepared by the embodiment can realize real-time and in-situ luminescent property regulation and control by randomly regulating and controlling the luminescent intensity of the upconversion luminescent material through temperature.
Experiments prove that the chemical general formula is A2-2x-2yEr2xYb2yW3O12On tungstate ofThe conversion luminescent material, when a is one or more of the elements Al, Bi, La, Gd, and Dy, also has a property that the position of the luminescence peak of the material does not change with the change of the luminescence intensity, but the luminescence intensity rapidly increases with the increase of the temperature.
Finally, the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all of them should be covered in the claims of the present invention.
Claims (6)
1. A tungstate up-conversion luminescent material is characterized in that the chemical general formula is A2-2x-2yEr2xYb2yW3O12Wherein A is element Y or Lu, 0<x+y<1；
The preparation method of the tungstate up-conversion luminescent material comprises the following steps:
a-containing compound, Er-containing compound, Yb-containing compound and W-containing compound were mixed according to A: er: yb: w = (2-2x-2 y): 2 x: 2 y: 3, pre-burning and grinding the mixture after the mixture is uniformly mixed, calcining the ground powder, cooling and grinding the powder to obtain the tungstate up-conversion luminescent material; wherein A is an element Y or Lu, 0< x + Y < 1; wherein: x =0.02 and y = 0.18.
2. The tungstate upconversion luminescent material of claim 1, wherein the particle size of the tungstate upconversion luminescent material is 0.2-100 μm.
3. The tungstate up-conversion luminescent material of claim 1, wherein the A-containing compound, the Er-containing compound, the Yb-containing compound, and the W-containing compound are selected from the group consisting of corresponding oxides, carbonates, oxalates, acetates, and compounds in the form of hydroxides.
4. The tungstate up-conversion luminescent material of claim 3, wherein the A-containing compound, the Er-containing compound, and the Yb-containing compound are each selected from the group consisting of corresponding oxides; the W-containing compound is WO3。
5. The tungstate up-conversion luminescent material of claim 1, wherein the A-containing compound, the Er-containing compound, the Yb-containing compound, and the W-containing compound are all 99.99% pure.
6. Use of a tungstate upconversion luminescent material, wherein the tungstate upconversion luminescent material is used in the fields of high-temperature upconversion imaging, temperature sensors and laser anti-counterfeiting according to any one of claims 1 to 5.
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